CN102653890A - Preparation method of highly-spinnable halogen-free flame-retardant nylon fiber - Google Patents
Preparation method of highly-spinnable halogen-free flame-retardant nylon fiber Download PDFInfo
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- CN102653890A CN102653890A CN2011100486302A CN201110048630A CN102653890A CN 102653890 A CN102653890 A CN 102653890A CN 2011100486302 A CN2011100486302 A CN 2011100486302A CN 201110048630 A CN201110048630 A CN 201110048630A CN 102653890 A CN102653890 A CN 102653890A
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- 229920001778 nylon Polymers 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000003063 flame retardant Substances 0.000 title abstract description 23
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title abstract description 11
- 239000004677 Nylon Substances 0.000 claims abstract description 44
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 16
- 238000009987 spinning Methods 0.000 claims abstract description 14
- 150000007974 melamines Chemical class 0.000 claims abstract description 13
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 11
- 238000002074 melt spinning Methods 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 238000005469 granulation Methods 0.000 claims abstract description 7
- 230000003179 granulation Effects 0.000 claims abstract description 7
- -1 cyclic phosphates Chemical class 0.000 claims abstract description 3
- 239000000835 fiber Substances 0.000 claims description 44
- 229920006052 Chinlon® Polymers 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 18
- 230000003078 antioxidant effect Effects 0.000 claims description 15
- 239000010452 phosphate Substances 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 10
- 229920000877 Melamine resin Polymers 0.000 claims description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 238000004381 surface treatment Methods 0.000 claims description 6
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical group CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 2
- 229920000388 Polyphosphate Polymers 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- ZJOLCKGSXLIVAA-UHFFFAOYSA-N ethene;octadecanamide Chemical compound C=C.CCCCCCCCCCCCCCCCCC(N)=O.CCCCCCCCCCCCCCCCCC(N)=O ZJOLCKGSXLIVAA-UHFFFAOYSA-N 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000001205 polyphosphate Substances 0.000 claims description 2
- 235000011176 polyphosphates Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000010456 wollastonite Substances 0.000 claims description 2
- 229910052882 wollastonite Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 7
- 229920000642 polymer Polymers 0.000 abstract description 5
- 235000021317 phosphate Nutrition 0.000 abstract 1
- 238000002485 combustion reaction Methods 0.000 description 10
- HVYLDJKDVOOTHV-UHFFFAOYSA-N acetic acid;2-iminoethanethiol Chemical compound CC(O)=O.CC(O)=O.SCC=N HVYLDJKDVOOTHV-UHFFFAOYSA-N 0.000 description 8
- 238000005453 pelletization Methods 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 239000004744 fabric Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 239000004952 Polyamide Substances 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 229920000784 Nomex Polymers 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010036 direct spinning Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004763 nomex Substances 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to a preparation method of highly-spinnable halogen-free flame-retardant nylon fibers, which comprises the following steps: performing blending and granulation of nylon slices, cyclic phosphates, melamine compounds, nanometer inorganic substances, and antioxidants in a double screw extruder to obtain a halogen-free flame-retardant nylon master batch, spinning the halogen-free flame-retardant nylon master batch with nylon slices into halogen-free flame-retardant nylon fibers through a melt spinning method. Compared with the prior art, the invention improves the dispersibility of the fire retardants and the compatibility of the polymers, and thus the product has good flame retardance; the spinnability of the nylon fibers is improved to a great extent; the invention has low cost, is industrialized; both halogen-free flame-retardant nylon aircraft seat covers and aviation carpet lines spun by the method of the invention pass FAR 25.853 cabin internal material flammability tests.
Description
Technical field
The present invention relates to a kind of fiber preparation method, especially relate to a kind of preparation method of high spinnability halogen-free flameproof nylon fibre.
Background technology
Nylon fibre is synthetic fiber of realizing suitability for industrialized production in the world the earliest.Although it does not include flammable fiber (limited oxygen index LOI=22～24), the existence of fusion dropping very easily causes spreading of fire during its burning, and is very unfavorable to fire control and disaster rescue.Owing to textiles catch fire or textiles not fire-retardant spread the fire that causes account for China in recent years fire incident 20%, fire-retardant fire-retardantization of macromolecular material progress one of field the most rapidly that become of textiles in recent years.
The production of flame-retardant textile has two kinds of methods, and the one, fabric is carried out flame-proof treatment promptly make fire retardant combine the purpose that reaches fire-retardant with fabric through rolling means such as baking process, rubbing method, spray-on process.Because the reactivity of nylon is low, fire retarding treating liquid is difficult to infiltrate fabric, and its flame retardant effect is along with the increase of service life and washing times reduces gradually, and the feel of fabric is poor, the weightening finish is bigger.
Another kind is to weave cotton cloth and have permanent fire retardant property with the fire resistance fibre direct spinning.Nylon fibre flame-retardant modified research beginning comparison early divides two kinds of copolymerization method and blending methods.Utilize copolymerization method,, thereby improved heat endurance through introducing aromatic ring or fragrant heterocycle in the macromolecular chain of fiber-forming polymer.Adopt this method; Du pont company and Japanese You Nijika company have successfully developed the aromatic series nylon fibre of commodity " Nomex " and " Apyil " by name respectively; Its heat resistance is very good; Limited oxygen index reaches 30～32, but because cost is high, so only be used for special dimensions such as military project, aerospace.Blending method promptly adds fire retardant in the melt of fiber-forming polymer or spinning solution; Method is simple; But fire retardant dispersed and can influence the spinnability of fiber with the compatibility of polymer, and for polyamide fibre, because the high temperature during hard to bear its fibers melt spinning of fire retardant causes the reduction of nylon fibre tensile strength; Be difficult to spinning continuously; Thereby the application that makes this method still is in lab scale and pilot scale stage, is in JP2010018906, JP2007308838, JP2007056392, JP2000328363,200710046218.0 these patents at application number, adopts different fire retardants to obtain fire-retardant nylon fibre; But all do not realize real high spinnability, no industrialized mass production.
Because the halogen-free flameproof nylon fibre can't suitability for industrialized production, at present China to produce and use be main with FLAME RETARDANT FINISH FABRIC still.Therefore there is above-mentioned various negative issue inevitably.
Summary of the invention
The object of the invention is exactly that a kind of preparation method that can realize industrialization, economical and practical high spinnability halogen-free flameproof nylon fibre is provided in order to overcome the defective that above-mentioned prior art exists.
The object of the invention can be realized through following technical scheme:
A kind of preparation method of high spinnability halogen-free flameproof nylon fibre is characterized in that, this method may further comprise the steps:
(1) with the blend granulation in double screw extruder of slices of caprone, annular phosphate, melamine compounds, nano-inorganic substance, antioxidant, obtains the halogen-free flameproof chinlon master batch;
(2) halogen-free flameproof chinlon master batch and slices of caprone are adopted melt spin processes and be spun into the halogen-free flameproof nylon fibre and get final product.
Halogen-free flameproof chinlon master batch described in the step (1) comprises following component and weight percent content:
Slices of caprone 45-60%;
Annular phosphate 5-8%;
Melamine compounds 30-45%;
Nano-inorganic substance 0.1-5%;
Antioxidant 1-2%.
Described slices of caprone uses the spinning level slices of caprone of viscosity as 2.8-3.4dl/g.
The ANTIBLAZE 1045 of the preferred AIBRIGHT & of described annular phosphate WILSON company.
Described melamine compounds is selected from melamine, melamine polyphosphate, MCA or melamine hydrobromate, preferred MCA.
Described melamine compounds carries out surface treatment through ethylene bis stearic acid amide (EBS) or glycerin monostearate (GMS), and 90% melamine compounds particle diameter is less than 5 microns, and wherein 50% melamine compounds particle diameter is the 1-2 micron.
The particle diameter of described nano-inorganic substance is 10nm-100nm.
Described nano-inorganic substance is calcium carbonate, barium sulfate, glass microballoon, kaolin, wollastonite, talcum powder, mica, imvite, aluminium hydroxide, magnesium hydroxide, diatomite or silica.
Described antioxidant is antioxidant 1098, antioxidant 1076 or antioxidant SEED.
The preferred antioxidant SEED of described antioxidant.
The mode that halogen-free flameproof chinlon master batch described in the step (2) and slices of caprone adopt weightless scale is added by following percentage by weight:
Slices of caprone 14-20%,
Halogen-free flameproof chinlon master batch 80-86%,
Described slices of caprone is that viscosity is the spinning level slices of caprone of 2.8-3.4dl/g.
The temperature of the melt spinning that melts spin processes described in the step (2) is a district 230-240 ℃, two district 240-245 ℃, and three district 240-245 ℃, 245 ℃ in four districts, spinning speed is 800-1200m/min, and drafting multiple is 3-4 times, and draft speed is 500m/min.
The halogen-free flameproof nylon fibre for preparing can be used in aircraft seat cover, aviation carpet line field.
Compared with prior art, the invention has the advantages that: since improve the dispersed of fire retardant and with the compatibility of polymer, not only have excellent flame-retardant performance; And improved the spinnability of nylon fibre to a great extent, and cost is low, has realized industrialization; But with this technology continuous spinning fracture of wire not more than 100 hours; Spinnable halogen-free flameproof nylon fibre specification is 8D, 15D, 20D, 30D, and limited oxygen index LOI is 31-32, halogen-free flameproof polyamide fibre aircraft seat cover and the aviation carpet line that obtains that spin; All passed through the flammable test of FAR 25.853 engine room inside materials; Average char length＜203mm behind the vertical combustion removes the average flame combustion time＜15s behind the burning things which may cause a fire disaster, the dropping average time＜5s that glows.
The specific embodiment
Below in conjunction with specific embodiment the present invention is elaborated.
Embodiment 1
The preparation of high spinnability halogen-free flameproof nylon fibre, first step halogen-free flameproof chinlon master batch wherein, each weight percentages of components is: slices of caprone (M2800; The Meida Company of meeting newly produces viscosity 2.8dl/g) 60%, annular phosphate (ANTIBLAZE 1045) 6%; MCA (through the EBS surface treatment) 30%; Wherein, 90% MCA particle diameter is less than 5 microns, and wherein 50% MCA particle diameter is the 1-2 micron; Nano diatomite (particle diameter is 10nm) 2%, antioxidant SEED 2%.Said components joins the parallel dual-screw extruding machine extruding pelletization after mixing, and with the pelletizing of tie rod water-cooled rear haulage, the double screw extruder temperature is set each district and is respectively 200 ℃-220 ℃-220 ℃-230 ℃-230 ℃-230 ℃-240 ℃-230 ℃.Cooling water temperature is controlled at 70 ℃, obtains the halogen-free flameproof chinlon master batch through melt extruding granulation and cooling off.
The preparation of the second step halogen-free flameproof nylon fibre; Adopt the mode of weightless scale to add halogen-free flameproof chinlon master batch and slices of caprone: slices of caprone (M2800 by following percentage by weight; The Meida Company of meeting newly produces viscosity 3.2dl/g) 14%, halogen-free flameproof chinlon master batch 86%.The temperature of its melt spinning is a district 230-240 ℃, two district 240-245 ℃, and three district 240-245 ℃, 245 ℃ in four districts, spinning speed is 1000m/min, and drafting multiple is 3 times, and draft speed is 500m/min; Spinnable halogen-free flameproof nylon fibre specification is 8D, 15D, 20D, 30D; Limited oxygen index LOI is 31.2; Through the flammable test of standard FAR 25.853 engine room inside materials; Average char length is 187mm behind the 12s vertical combustion, removes the average flame combustion time 11s behind the burning things which may cause a fire disaster, dropping 4.3s average time that glows.This halogen-free flameproof nylon fibre has been used for the non-halogen project of Boeing jumbo carpet, the small lot use of Italian Aquafil company.
Embodiment 2
The preparation of high spinnability halogen-free flameproof nylon fibre, first step halogen-free flameproof chinlon master batch wherein, each weight percentages of components is: slices of caprone (M3200; The Meida Company of meeting newly produces viscosity 3.2dl/g) 45%, annular phosphate (ANTIBLAZE 1045) 5%; MCA 45%, wherein, 90% MCA particle diameter is less than 5 microns; Wherein 50% MCA particle diameter is the 1-2 micron; Nano imvite (through the EBS surface treatment, particle diameter is 50nm) 4%, antioxidant SEED 1%.Said components joins the parallel dual-screw extruding machine extruding pelletization after mixing, and with the pelletizing of tie rod water-cooled rear haulage, the double screw extruder temperature is set each district and is respectively 200 ℃-220 ℃-220 ℃-230 ℃-230 ℃-230 ℃-240 ℃-230 ℃.Cooling water temperature is controlled at 70 ℃, obtains the halogen-free flameproof chinlon master batch through melt extruding granulation and cooling off.
The preparation of the second step halogen-free flameproof nylon fibre; Adopt the mode of weightless scale to add halogen-free flameproof chinlon master batch and slices of caprone: slices of caprone (M2800 by following percentage by weight; The Meida Company of meeting newly produces viscosity 3.4dl/g) 20%, halogen-free flameproof chinlon master batch 80%.The temperature of its melt spinning is a district 230-240 ℃, two district 240-245 ℃, and three district 240-245 ℃, 245 ℃ in four districts, spinning speed is 800m/min, and drafting multiple is 3.2 times, and draft speed is 500m/min; Spinnable halogen-free flameproof nylon fibre specification is 8D, 15D, 20D, 30D; Limited oxygen index LOI is 31.9; Through the flammable test of standard FAR 25.853 engine room inside materials; Average char length is 156mm behind the 12s vertical combustion, removes the average flame combustion time 5s behind the burning things which may cause a fire disaster, dropping 3.2s average time that glows.
Embodiment 3
The preparation of high spinnability halogen-free flameproof nylon fibre, first step halogen-free flameproof chinlon master batch wherein, each weight percentages of components is: slices of caprone (M3200; The Meida Company of meeting newly produces viscosity 3.2dl/g) 48%, annular phosphate (ANTIBLAZE 1045) 7%; MCA (through the GMS surface treatment) 42.9%; Wherein, 90% MCA particle diameter is less than 5 microns, and wherein 50% MCA particle diameter is the 1-2 micron; Nano-glass microballon (particle diameter is 100nm) 0.1%, antioxidant SEED2%.Said components joins the parallel dual-screw extruding machine extruding pelletization after mixing, and with the pelletizing of tie rod water-cooled rear haulage, the double screw extruder temperature is set each district and is respectively 200 ℃-220 ℃-220 ℃-230 ℃-230 ℃-230 ℃-240 ℃-230 ℃.Cooling water temperature is controlled at 80 ℃, obtains the halogen-free flameproof chinlon master batch through melt extruding granulation and cooling off.
The preparation of the second step halogen-free flameproof nylon fibre; Adopt the mode of weightless scale to add halogen-free flameproof chinlon master batch and slices of caprone: slices of caprone (M2800 by following percentage by weight; The Meida Company of meeting newly produces viscosity 3.0dl/g) 18%, halogen-free flameproof chinlon master batch 82%.The temperature of its melt spinning is a district 230-240 ℃, two district 240-245 ℃, and three district 240-245 ℃, 245 ℃ in four districts, spinning speed is 1200m/min, and drafting multiple is 3.6 times, and draft speed is 500m/min; Spinnable halogen-free flameproof nylon fibre specification is 8D, 15D, 20D, 30D; Limited oxygen index LOI is 31.5; Through the flammable test of standard FAR 25.853 engine room inside materials; Average char length is 167mm behind the 12s vertical combustion, removes the average flame combustion time 6s behind the burning things which may cause a fire disaster, dropping 3.5s average time that glows.
Embodiment 4
The preparation of high spinnability halogen-free flameproof nylon fibre, first step halogen-free flameproof chinlon master batch wherein, each weight percentages of components is: slices of caprone (M3400; The Meida Company of meeting newly produces viscosity 3.4dl/g) 51%, annular phosphate (ANTIBLAZE 1045) 8%; Melamine hydrobromate (through the EBS surface treatment) 35%; Wherein, 90% melamine hydrobromate particle diameter is less than 5 microns, and wherein 50% melamine hydrobromate particle diameter is the 1-2 micron; Nano barium sulfate (particle diameter is 70nm) 5%, antioxidant SEED 1%.Said components joins the parallel dual-screw extruding machine extruding pelletization after mixing, and with the pelletizing of tie rod water-cooled rear haulage, the double screw extruder temperature is set each district and is respectively 200 ℃-220 ℃-220 ℃-230 ℃-230 ℃-230 ℃-240 ℃-230 ℃.Cooling water temperature is controlled at 60 ℃, obtains the halogen-free flameproof chinlon master batch through melt extruding granulation and cooling off.
The preparation of the second step halogen-free flameproof nylon fibre; Adopt the mode of weightless scale to add halogen-free flameproof chinlon master batch and slices of caprone: slices of caprone (M2800 by following percentage by weight; The Meida Company of meeting newly produces viscosity 2.8dl/g) 16%, halogen-free flameproof chinlon master batch 84%.The temperature of its melt spinning is a district 230-240 ℃, two district 240-245 ℃, and three district 240-245 ℃, 245 ℃ in four districts, spinning speed is 1100m/min, and drafting multiple is 3.5 times, and draft speed is 500m/min; Spinnable halogen-free flameproof nylon fibre specification is 8D, 15D, 20D, 30D; Limited oxygen index LOI is 31.2; Through the flammable test of standard FAR 25.853 engine room inside materials; Average char length is 181mm behind the 12s vertical combustion, removes the average flame combustion time 8s behind the burning things which may cause a fire disaster, dropping 3.9s average time that glows.
Claims (10)
1. the preparation method of one kind high spinnability halogen-free flameproof nylon fibre is characterized in that, this method may further comprise the steps:
(1) with the blend granulation in double screw extruder of slices of caprone, annular phosphate, melamine compounds, nano-inorganic substance, antioxidant, obtains the halogen-free flameproof chinlon master batch;
(2) halogen-free flameproof chinlon master batch and slices of caprone are adopted melt spin processes and be spun into the halogen-free flameproof nylon fibre and get final product.
2. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 1 is characterized in that, the halogen-free flameproof chinlon master batch described in the step (1) comprises following component and weight percent content:
Slices of caprone 45-60%;
Annular phosphate 5-8%;
Melamine compounds 30-45%;
Nano-inorganic substance 0.1-5%;
Antioxidant 1-2%.
3. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 2 is characterized in that, described slices of caprone uses the spinning level slices of caprone of viscosity as 2.8-3.4dl/g.
4. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 2 is characterized in that, the ANTIBLAZE 1045 of the preferred AIBRIGHT & of described annular phosphate WILSON company.
5. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 2; It is characterized in that; Described melamine compounds is selected from melamine, melamine polyphosphate, MCA or melamine hydrobromate, preferred MCA.
6. according to the preparation method of claim 2 or 5 described a kind of high spinnability halogen-free flameproof nylon fibres; It is characterized in that; Described melamine compounds carries out surface treatment through ethylene bis stearic acid amide (EBS) or glycerin monostearate (GMS); 90% melamine compounds particle diameter is less than 5 microns, and wherein 50% melamine compounds particle diameter is the 1-2 micron.
7. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 2; It is characterized in that; Described nano-inorganic substance is calcium carbonate, barium sulfate, glass microballoon, kaolin, wollastonite, talcum powder, mica, imvite, aluminium hydroxide, magnesium hydroxide, diatomite or silica, and particle diameter is 10nm-100nm.
8. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 2 is characterized in that, described antioxidant is antioxidant 1098, antioxidant 1076 or antioxidant SEED, preferred antioxidant SEED.
9. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 1 is characterized in that, halogen-free flameproof chinlon master batch described in the step (2) and slices of caprone add by following percentage by weight:
Slices of caprone 14-20%,
Halogen-free flameproof chinlon master batch 80-86%,
Wherein slices of caprone is that viscosity is the spinning level slices of caprone of 2.8-3.4dl/g.
10. the preparation method of a kind of high spinnability halogen-free flameproof nylon fibre according to claim 1 is characterized in that, the temperature of the melt spinning that melts spin processes described in the step (2) is a district 230-240 ℃; Two district 240-245 ℃; Three district 240-245 ℃, 245 ℃ in four districts, spinning speed is 800-1200m/min; Drafting multiple is 3-4 times, and draft speed is 500m/min.
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| CN201110048630.2A CN102653890B (en) | 2011-03-01 | 2011-03-01 | Preparation method of highly-spinnable halogen-free flame-retardant nylon fiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103173932A (en) * | 2013-03-20 | 2013-06-26 | 天津工业大学 | Preparation method of antiflaming cellulose non-woven cloth |
| CN103276530A (en) * | 2013-05-10 | 2013-09-04 | 安徽一隆羽绒有限公司 | Flame retarding down feather and feather fiber combined feather cotton and manufacturing method thereof |
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| CN103613556A (en) * | 2013-10-18 | 2014-03-05 | 上海美莱珀化工材料科技有限公司 | Tripolycyanamide hydrobromide and preparation method thereof |
| CN103882548A (en) * | 2012-12-20 | 2014-06-25 | 辽宁银珠化纺集团有限公司 | Functional nylon 66 fiber and preparation method thereof |
| CN104558681A (en) * | 2015-01-30 | 2015-04-29 | 江苏弘盛新材料股份有限公司 | Flame retardant and application thereof in thermal-oxidation-resistant flame-retardant nylon 6 |
| CN105088385A (en) * | 2015-09-02 | 2015-11-25 | 太仓市宏亿化纤有限公司 | Flame-retarding polyamide fabric and preparation method thereof |
| CN106192055A (en) * | 2016-08-09 | 2016-12-07 | 福建万鸿纺织有限公司 | A kind of high-elastic fire-retardant chinlon |
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| CN109881287A (en) * | 2019-01-28 | 2019-06-14 | 圣华盾防护科技股份有限公司 | A kind of flame-retardant wear-resistant protective article and fiber |
| CN110656394A (en) * | 2019-10-23 | 2020-01-07 | 东华大学 | Schiff base P-N-Si flame-retardant PA6, fiber and preparation method thereof |
| CN111574828A (en) * | 2020-06-30 | 2020-08-25 | 上海芷燃新材料有限公司 | Nylon halogen-free flame-retardant master batch and preparation method thereof |
| CN111676540A (en) * | 2020-07-03 | 2020-09-18 | 南通文凯化纤有限公司 | Flame-retardant polyamide filament and preparation method thereof |
| CN112779619A (en) * | 2021-03-26 | 2021-05-11 | 北京邦维高科特种纺织品有限责任公司 | Polyamide flame-retardant fiber and product thereof |
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| CN114197077A (en) * | 2021-11-26 | 2022-03-18 | 厦门稀土材料研究所 | A kind of rare earth flame retardant nylon fiber and preparation method thereof |
| CN114606586A (en) * | 2022-03-17 | 2022-06-10 | 浙江四通新材料科技股份有限公司 | A kind of halogen-free and phosphorus-free flame retardant nylon and preparation method thereof |
| CN117343497A (en) * | 2023-09-25 | 2024-01-05 | 苏州宝丽迪材料科技股份有限公司 | Halogen-free flame-retardant master batch for polyester fiber, and preparation method and application thereof |
| CN118745606A (en) * | 2024-07-29 | 2024-10-08 | 威海海马科创纤维有限公司 | A method for preparing flame-retardant carpet yarn from waste nylon fibers |
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| CN103882548B (en) * | 2012-12-20 | 2016-08-24 | 辽宁银珠化纺集团有限公司 | A kind of functional type nylon 66 fiber and preparation method thereof |
| CN103882548A (en) * | 2012-12-20 | 2014-06-25 | 辽宁银珠化纺集团有限公司 | Functional nylon 66 fiber and preparation method thereof |
| CN103173932A (en) * | 2013-03-20 | 2013-06-26 | 天津工业大学 | Preparation method of antiflaming cellulose non-woven cloth |
| CN103276530B (en) * | 2013-05-10 | 2016-03-02 | 安徽一隆羽绒有限公司 | Feather cotton that fire-retardant eider down, feather fiber combine and preparation method thereof |
| CN103276530A (en) * | 2013-05-10 | 2013-09-04 | 安徽一隆羽绒有限公司 | Flame retarding down feather and feather fiber combined feather cotton and manufacturing method thereof |
| CN103435952B (en) * | 2013-07-30 | 2015-08-05 | 浙江万盛股份有限公司 | A kind of Phosphate nano composite flame-retardant masterbatch and preparation method thereof |
| CN103435952A (en) * | 2013-07-30 | 2013-12-11 | 浙江万盛股份有限公司 | Phosphate nano composite flame-retardant masterbatch and preparation method thereof |
| CN103613556A (en) * | 2013-10-18 | 2014-03-05 | 上海美莱珀化工材料科技有限公司 | Tripolycyanamide hydrobromide and preparation method thereof |
| CN104558681A (en) * | 2015-01-30 | 2015-04-29 | 江苏弘盛新材料股份有限公司 | Flame retardant and application thereof in thermal-oxidation-resistant flame-retardant nylon 6 |
| CN105088385A (en) * | 2015-09-02 | 2015-11-25 | 太仓市宏亿化纤有限公司 | Flame-retarding polyamide fabric and preparation method thereof |
| CN106192055A (en) * | 2016-08-09 | 2016-12-07 | 福建万鸿纺织有限公司 | A kind of high-elastic fire-retardant chinlon |
| CN106929939B (en) * | 2017-03-02 | 2019-06-28 | 上海市合成纤维研究所有限公司 | A kind of Jinlun-6 fireproof fiber and preparation method thereof |
| CN106929939A (en) * | 2017-03-02 | 2017-07-07 | 上海市合成纤维研究所有限公司 | A kind of Jinlun-6 fireproof fiber and preparation method thereof |
| CN108070936A (en) * | 2017-12-06 | 2018-05-25 | 三橡股份有限公司 | A kind of Train brake hose nylon fibre, preparation method and the usage |
| CN108728925A (en) * | 2018-06-29 | 2018-11-02 | 南通文凯化纤有限公司 | A kind of preparation method of halogen-free flameproof nylon fibre |
| CN109881287A (en) * | 2019-01-28 | 2019-06-14 | 圣华盾防护科技股份有限公司 | A kind of flame-retardant wear-resistant protective article and fiber |
| CN109881287B (en) * | 2019-01-28 | 2022-03-18 | 圣华盾防护科技股份有限公司 | A kind of flame-retardant wear-resistant protective article and fiber |
| CN110656394A (en) * | 2019-10-23 | 2020-01-07 | 东华大学 | Schiff base P-N-Si flame-retardant PA6, fiber and preparation method thereof |
| CN110656394B (en) * | 2019-10-23 | 2021-08-10 | 东华大学 | Schiff base P-N-Si flame-retardant PA6, fiber and preparation method thereof |
| CN111574828A (en) * | 2020-06-30 | 2020-08-25 | 上海芷燃新材料有限公司 | Nylon halogen-free flame-retardant master batch and preparation method thereof |
| CN111676540A (en) * | 2020-07-03 | 2020-09-18 | 南通文凯化纤有限公司 | Flame-retardant polyamide filament and preparation method thereof |
| CN112941642A (en) * | 2021-01-12 | 2021-06-11 | 浙江古纤道绿色纤维有限公司 | Colored slice mixing method |
| CN112779619B (en) * | 2021-03-26 | 2022-01-28 | 北京邦维高科新材料科技股份有限公司 | Polyamide flame-retardant fiber and product thereof |
| CN112779619A (en) * | 2021-03-26 | 2021-05-11 | 北京邦维高科特种纺织品有限责任公司 | Polyamide flame-retardant fiber and product thereof |
| CN114197077A (en) * | 2021-11-26 | 2022-03-18 | 厦门稀土材料研究所 | A kind of rare earth flame retardant nylon fiber and preparation method thereof |
| CN114197077B (en) * | 2021-11-26 | 2023-07-11 | 厦门稀土材料研究所 | Rare earth flame-retardant nylon fiber and preparation method thereof |
| CN114606586A (en) * | 2022-03-17 | 2022-06-10 | 浙江四通新材料科技股份有限公司 | A kind of halogen-free and phosphorus-free flame retardant nylon and preparation method thereof |
| CN117343497A (en) * | 2023-09-25 | 2024-01-05 | 苏州宝丽迪材料科技股份有限公司 | Halogen-free flame-retardant master batch for polyester fiber, and preparation method and application thereof |
| CN118745606A (en) * | 2024-07-29 | 2024-10-08 | 威海海马科创纤维有限公司 | A method for preparing flame-retardant carpet yarn from waste nylon fibers |
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